JPH10167854A - Production of high strength porous alpha-sic sintered compact - Google Patents
Production of high strength porous alpha-sic sintered compactInfo
- Publication number
- JPH10167854A JPH10167854A JP8332167A JP33216796A JPH10167854A JP H10167854 A JPH10167854 A JP H10167854A JP 8332167 A JP8332167 A JP 8332167A JP 33216796 A JP33216796 A JP 33216796A JP H10167854 A JPH10167854 A JP H10167854A
- Authority
- JP
- Japan
- Prior art keywords
- sic
- content
- weight
- sintered body
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/067—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Ceramic Products (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、α−SiＣ焼結体の
製造方法に関し、特に、ハニカムフィルタ等を製造する
に適した濾過性能の良好な高強度多孔質α−SiＣ焼結体
の製造方法について提案する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an .alpha.-SiC sintered body, and more particularly, to a method for producing a high-strength porous .alpha.-SiC sintered body having good filtration performance suitable for producing a honeycomb filter or the like. Suggest a way.
【０００２】[0002]
【従来の技術】最近、ディーゼルエンジンの内燃機関な
どから排出される排気ガス中に含まれるパティキュレー
ト (カーボンの粒子状物質) については、環境浄化を図
る観点から、ガスの大気放出の前に除去するのが普通で
ある。この除去のために用いられているのがセラミック
フィルタである。このセラミックフィルタに求められて
いる資質としては、耐熱性, 熱伝導性に優れることであ
り、こうした条件に適うものとして多孔質のSiＣ焼結体
の適用が検討されている。2. Description of the Related Art Recently, particulates (particulate matter of carbon) contained in exhaust gas discharged from an internal combustion engine of a diesel engine or the like are removed before releasing the gas to the atmosphere from the viewpoint of environmental purification. It is usual to do. A ceramic filter is used for this removal. The qualities required of the ceramic filter are excellent in heat resistance and thermal conductivity, and application of a porous SiC sintered body is being studied as meeting such conditions.
【０００３】従来、多孔質SiＣ焼結体は、β−SiＣ粉末
に有機樹脂バインダーおよび可塑剤等を配合した原料組
成物を成形し、その成形体を焼成することによりβ−Si
Ｃ粉末粒子を粒成長させて板状結晶を生成させたのち、
焼結することによって製造していた。このような板状結
晶組織を有するβ−SiＣ焼結体は、気孔率が大きく、排
ガスフィルターとして使用した場合の圧力損失 (または
排気抵抗) が低いという特徴がある。Conventionally, a porous SiC sintered body is obtained by molding a raw material composition in which an organic resin binder, a plasticizer, and the like are mixed with β-SiC powder, and firing the molded body to form a β-SiC powder.
After growing C powder particles to form plate crystals,
It was manufactured by sintering. The β-SiC sintered body having such a plate-like crystal structure is characterized by high porosity and low pressure loss (or exhaust resistance) when used as an exhaust gas filter.
【０００４】しかしながら、このβ−SiＣ焼結体は、焼
結時に粒の異常成長が起こりやすく、そのために均一で
かつ所定の気孔径を有する焼結体とするためには、極め
て狭い温度範囲内に制御することが必要である。さらに
この方法で得られたβ−SiＣ焼結体は、主として板状結
晶で構成されるため、機械的強度が比較的低いという問
題があった。However, in the β-SiC sintered body, abnormal growth of grains is apt to occur during sintering. Therefore, in order to obtain a sintered body having a uniform and predetermined pore diameter, an extremely narrow temperature range is required. Needs to be controlled. Further, the β-SiC sintered body obtained by this method has a problem that the mechanical strength is relatively low because it is mainly composed of plate crystals.
【０００５】また、特開平４−１８７５７８号公報に
は、セラミックフィルタに用いることのできる多孔質Si
Ｃ焼結体の製造方法として、β−SiＣ粉末にαーSiＣ粉
末を配合したSiＣ原料粉末を成形し、その成形体を焼成
して多孔質SiＣ焼結体とする方法において、上記SiＣ原
料粉末が、平均粒径 0.1〜1.0 μｍのβ−SiＣ粉末 100
重量部に対し、平均粒径が 0.3〜50μｍのα−SiＣ粉末
を５〜５０重量部配合する多孔質SiＣ焼結体の製造方法
が開示されている。しかしながら、β−SiＣ粉末を多量
に使用する上記の方法で製造された多孔質SiＣ焼結体
は、β−SiＣ粉末が高価であることから多孔質SiＣ焼結
体はそれほど安価にはならず、また、β−SiＣ粉末は、
焼結時に板状の結晶粒を生成するため比較的気孔径が大
きくなり易く、通気抵抗の比較的小さいフィルタを製造
することができるが、気孔径分布が不均一になり易いと
いう問題があった。Japanese Patent Laid-Open No. Hei 4-187578 discloses a porous Si filter which can be used for a ceramic filter.
As a method for producing a C sintered body, the method comprises molding a SiC raw material powder obtained by blending an α-SiC powder with a β-SiC powder, and firing the formed body to form a porous SiC sintered body. Is a β-SiC powder having an average particle size of 0.1 to 1.0 μm.
There is disclosed a method for producing a porous SiC sintered body in which 5 to 50 parts by weight of α-SiC powder having an average particle diameter of 0.3 to 50 μm is blended with respect to parts by weight. However, the porous SiC sintered body manufactured by the above method using a large amount of β-SiC powder is not so inexpensive because the β-SiC powder is expensive. Also, β-SiC powder is
Since sintering produces plate-like crystal grains, the pore size is relatively large, and a filter having relatively small airflow resistance can be manufactured. However, there is a problem that the pore size distribution tends to be non-uniform. .
【０００６】[0006]
【発明が解決しようとする課題】本発明は、従来のハニ
カムフィルタ用多孔質β−SiＣ焼結体が抱えている上述
した問題を解決するために開発されたものであって、そ
の目的とするところは、通気抵抗が小さくかつ均一な気
孔径分布を有するハニカムフィルタ用多孔質α−SiＣ焼
結体を提供することにある。また、本発明の他の目的
は、有機樹脂バインダーを添加して高強度のα−SiＣ焼
結体を安価に製造することにある。SUMMARY OF THE INVENTION The present invention has been developed to solve the above-mentioned problems of the conventional porous β-SiC sintered body for a honeycomb filter. However, an object of the present invention is to provide a porous α-SiC sintered body for a honeycomb filter having a small airflow resistance and a uniform pore size distribution. Another object of the present invention is to produce an α-SiC sintered body having high strength at low cost by adding an organic resin binder.
【０００７】[0007]
【課題を解決するための手段】上述した課題について検
討した結果、その解決のためには、SiO2含有率が 0.1〜
５重量％で平均粒径が 0.3〜50μｍのSiＣ原料粉末に有
機樹脂バインダーを添加混合して成形し、その成形体を
酸素含有率が１〜10％の雰囲気中において該成形体中の
熱分解炭素含有率が 0.5〜５重量％となるように加熱し
た後、該成形体を1500〜2500℃の非酸化性雰囲気中で焼
成することが高強度多孔質α−SiＣ焼結体の製造に有利
であるとの結論に達した。なお、前記SiＣ原料粉末とし
ては、α−SiＣの含有率が60〜100 ％のものを用いるこ
とが好ましい。As a result of studying the above-mentioned problems, it has been found that the content of SiO 2 is 0.1 to
An organic resin binder is added to and mixed with a 5% by weight SiC raw material powder having an average particle size of 0.3 to 50 μm, and the molded product is thermally decomposed in an atmosphere having an oxygen content of 1 to 10%. After heating to a carbon content of 0.5 to 5% by weight, firing the molded body in a non-oxidizing atmosphere at 1500 to 2500 ° C. is advantageous for producing a high-strength porous α-SiC sintered body. Was reached. The SiC raw material powder preferably has a content of α-SiC of 60 to 100%.
【０００８】[0008]
【発明の実施の形態】本発明において、成形体中にSiO2
と有機樹脂バインダーからの適量の熱分解炭素とを存在
させるようにした理由は、成形体中にSiO2とＣとが適量
存在すると、その後の焼結過程で発生するSiＯガスが焼
結に関与する際に、SiＣ粒子を粗大化させることなく比
較的容易に相互に結合させることができるようになるか
らである。これは、SiＣ原料粉末としてα−SiＣ粉末を
多量に使うことと相俟って本発明の効果をより一層顕著
なものにするのに役立っている。BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, SiO 2
The reason that so as to present the appropriate amount of pyrolytic carbon from the organic resin binder, when the SiO 2 and C present an appropriate amount in the green body, SiO gas generated in the subsequent sintering process is involved in sintering This is because SiC particles can be relatively easily bonded to each other without coarsening. This, together with the use of a large amount of α-SiC powder as the SiC raw material powder, has helped to make the effects of the present invention more remarkable.
【０００９】一般に、SiO2とＣとからSiＣが生成する反
応は、下記式； SiO2＋Ｃ→SiＯ＋ＣＯ SiＯ＋２Ｃ→SiＣ＋ＣＯ に従って、まずSiＯが生成し、次いでこのSiＯとＣとが
反応してSiＣを生成するものと考えられている。ここ
で、そのSiO2とＣとの配合が不適当だと、SiＯガスのう
ちSiＣ化されないものが多くなり、反応域中のSiＯガス
量が増加し、SiO2, Si, SiＣ, Ｃが混合した粘着性の半
溶融物を析出して原料の凝着を招く。しかし、この配合
が適正だと高強度多孔質SiＣの生成を容易に起こさせる
ことができる。In general, the reaction for forming SiC from SiO 2 and C is as follows: SiO 2 + C → SiO + CO SiO + 2C → SiC + CO First, SiO is formed, and then the SiO and C react to form SiC. It is considered to be. Here, if the mixing ratio of SiO 2 and C is inappropriate, many of the SiO gases that cannot be converted to SiC increase, the amount of SiO gas in the reaction zone increases, and SiO 2 , Si, SiC, and C are mixed. The adhered sticky semi-molten substance is precipitated to cause adhesion of the raw materials. However, if this composition is proper, the formation of high-strength porous SiC can be easily caused.
【００１０】上記の反応を適正に保つための前記SiＣ原
料粉末中には、0.1 〜5 重量％のSiO2を含有させること
が適当である。この理由は、SiO2含有率が0.1 重量％よ
り小さいと、焼成過程で発生するSiＯガスが少なくな
り、SiＣ粒子を粒成長させることなく相互に結合させる
ことが困難になるからである。一方、５重量％より大き
いと、焼成過程で発生するＣＯガスとSiＯガスが多くな
りすぎ、上述したように焼結反応を阻害するからであ
る。なお、好ましいSiO2含有率は 0.3〜2.0 重量％であ
る。より好適には 1.0〜2.0 重量％がよい。It is appropriate that the SiC raw material powder contains 0.1 to 5% by weight of SiO 2 in order to maintain the above reaction properly. The reason for this is that if the SiO 2 content is less than 0.1% by weight, the amount of SiO gas generated during the sintering process will be small, and it will be difficult to bond the SiC particles to each other without causing grain growth. On the other hand, if it is more than 5% by weight, the amount of CO gas and SiO gas generated during the firing process becomes too large, which hinders the sintering reaction as described above. The preferred SiO 2 content is 0.3 to 2.0% by weight. More preferably, the content is 1.0 to 2.0% by weight.
【００１１】前記SiＣ原料粉末は、平均粒径が0.3 〜50
μｍの大きさであることが必要である。この理由は、平
均粒径が0.3 〜50μｍのSiＣ原料粉末を使用することに
よって、通気抵抗が小さく、かつ、均一な気孔径分布を
有するハニカムフィルタ等に適した高強度多孔質α−Si
Ｃ焼結体を安価に提供することができるからである。The SiC raw material powder has an average particle size of 0.3 to 50.
It is necessary to have a size of μm. The reason for this is that the use of SiC raw material powder having an average particle size of 0.3 to 50 μm makes it possible to obtain a high-strength porous α-Si film having a small airflow resistance and suitable for a honeycomb filter having a uniform pore size distribution.
This is because a C sintered body can be provided at low cost.
【００１２】原料粉末である前記SiＣ原料粉末として
は、α−SiＣ含有率が60〜100 ％のものを用いることが
好ましい。その理由は、α−SiＣ含有率が60％より低い
と、β−SiＣ等の焼結時に異常粒成長しやすい成分の影
響で、成形体の焼結時に板状の結晶粒が生成し易くな
り、気孔径分布が不均一になり易いからである。As the SiC raw material powder, it is preferable to use one having an α-SiC content of 60 to 100%. The reason is that if the α-SiC content is lower than 60%, plate-like crystal grains are likely to be generated at the time of sintering of the molded body due to the influence of components such as β-SiC which tend to grow abnormal grains during sintering. This is because the pore size distribution tends to be non-uniform.
【００１３】本発明において、SiＣ原料粉末には、有機
質樹脂からなる結合剤, 即ち、有機樹脂バインダーを添
加混合して成形し、その後、酸素含有率が１〜10％の雰
囲気中で熱分解炭素含有率が0.5 〜５重量％となるまで
有機質樹脂を熱分解させることが必要である。かかる有
機樹脂バインダーは、熱分解温度以上に加熱された場合
にＣを析出する有機質化合物であって、その生成Ｃ量
は、SiＣに含有されるSiO2を除去するために用いられる
量とする。従って、この有機樹脂バインダーは、少なく
ともSiO2含有率に見合う量、即ちSiO2をSiＣ化すること
のできる量とし、できればSiＣ粒子間に均一に介在する
に充分な量を添加する。In the present invention, a binder made of an organic resin, that is, an organic resin binder is added to the SiC raw material powder, mixed and molded, and then the pyrolytic carbon is mixed in an atmosphere having an oxygen content of 1 to 10%. It is necessary to thermally decompose the organic resin until the content becomes 0.5 to 5% by weight. Such an organic resin binder is an organic compound that precipitates C when heated to a temperature equal to or higher than the thermal decomposition temperature, and the amount of generated C is an amount used for removing SiO 2 contained in SiC. Therefore, the organic resin binder is at least an amount commensurate with the SiO 2 content, i.e. the SiO 2 and the amount that can be SiC of, adding an amount sufficient to uniformly interposed between SiC particles, if possible.
【００１４】つまり、本発明は、前記有機樹脂バインダ
ーを、SiＣ原料粉末ならびに反応域酸素含有量によって
必要とされる量よりもやや過剰に添加し、積極的にSiＣ
焼結体内に遊離炭素の形で残留させることで、高強度で
均一気孔径を有する多孔質α−SiＣ焼結体を生成させよ
うとするものである。That is, according to the present invention, the organic resin binder is added slightly in excess of the amount required according to the SiC raw material powder and the oxygen content in the reaction zone, and the SiC binder is aggressively added.
By leaving it in the form of free carbon in the sintered body, a porous α-SiC sintered body having a high strength and a uniform pore diameter is to be produced.
【００１５】本発明において、雰囲気中の酸素含有率を
１〜10％に制御する理由は、雰囲気中の酸素含有率が１
％より低いと反応性の高い熱分解炭素を得ることが困難
になるからであり、一方10％より高いと有機樹脂バイン
ダーが燃焼して反応性の高い熱分解炭素を得ることがで
きないからである。In the present invention, the reason that the oxygen content in the atmosphere is controlled to 1 to 10% is that the oxygen content in the atmosphere is 1%.
If the amount is less than 10%, it becomes difficult to obtain highly reactive pyrolytic carbon, while if it is more than 10%, the organic resin binder burns and it is not possible to obtain highly reactive pyrolytic carbon. .
【００１６】また、成形体中の熱分解炭素含有率を 0.5
〜５重量％にする理由は、この熱分解炭素の含有率が
0.5重量％より少ないと、SiＣ粒子を粗大化させること
なく相互に結合させることが困難になるからであり、一
方５重量％より多いとSiＣ粒子間に存在する熱分解炭素
がSiＣ粒子の相互の結合を阻害するからである。Further, the pyrolytic carbon content in the compact is 0.5
The reason for setting the content to 5% by weight is that the content of the pyrolytic carbon is
If the amount is less than 0.5% by weight, it is difficult to bond the SiC particles to each other without coarsening. On the other hand, if the amount is more than 5% by weight, the pyrolytic carbon existing between the SiC particles may cause mutual decomposition of the SiC particles. This is because binding is inhibited.
【００１７】なお、本発明において用いる前記有機樹脂
バインダーとしては、メチルセルロース、カルボキシメ
チルセルロース、ヒドロキシエチルセルロース、ポリエ
チレングリコール、フェノール樹脂、エポキシ樹脂等が
あげられる。この成形用バインダーの配合割合は一般
に、SiＣ原料粉末 100重量部に対し、1 〜10重量部の範
囲が好適である。この配合割合が1 重量部未満では、必
要な熱分解炭素の生成量が得られないからであり、一方
10重量部を超えると、バインダーを除去する際に成形体
にクラックが発生し易くなる。The organic resin binder used in the present invention includes methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyethylene glycol, phenol resin, epoxy resin and the like. In general, the compounding ratio of the molding binder is preferably in the range of 1 to 10 parts by weight based on 100 parts by weight of the SiC raw material powder. If the blending ratio is less than 1 part by weight, the required amount of generated pyrolytic carbon cannot be obtained.
If the amount exceeds 10 parts by weight, cracks are likely to occur in the molded article when the binder is removed.
【００１８】前記原料粉末には必要に応じて分散溶媒を
配合する。例えば、ベンゼン等の有機溶剤、メタノール
等のアルコール、水等が使用することができ、その配合
量は原料スラリーの粘度に応じて調整される。A dispersion solvent is added to the raw material powder as required. For example, organic solvents such as benzene, alcohols such as methanol, water, and the like can be used, and the compounding amount is adjusted according to the viscosity of the raw material slurry.
【００１９】本発明において、焼結時の成形体の焼成雰
囲気を非酸化性雰囲気とする理由は、SiＣの酸化による
必要以上のSiO2の生成を防ぐためであり、その温度は15
00〜2500℃の範囲内とする。焼成雰囲気の温度が1500℃
未満では、SiＣ粒子の焼結が進行しないからであり、一
方2500℃を超えるとSiＣが昇華するためである。好まし
くは1800〜2300℃の範囲とする。本発明によれば、壁厚
が 0.2〜0.5 mmで、軸方向に 100〜250 個／平方インチ
の割合で多数の孔が形成され、100 mm以上の長さを有す
るハニカム形状のフィルターを有利に製造することがで
きる。In the present invention, the reason why the firing atmosphere of the compact during sintering is a non-oxidizing atmosphere is to prevent the generation of unnecessarily SiO 2 due to the oxidation of SiC.
The temperature is in the range of 00 to 2500 ° C. Temperature of firing atmosphere is 1500 ℃
If it is less than the above, the sintering of the SiC particles does not proceed, while if it exceeds 2500 ° C., the SiC will sublime. Preferably it is in the range of 1800 to 2300 ° C. According to the present invention, a honeycomb-shaped filter having a wall thickness of 0.2 to 0.5 mm, a large number of holes formed at a rate of 100 to 250 holes / square inch in the axial direction, and a length of 100 mm or more is advantageously used. Can be manufactured.
【００２０】[0020]
【実施例】以下に、本発明を内燃機関の排気ガス浄化装
置に使用するフィルターの形状に具体化した実施例を比
較例と対比させて説明する。なお、このフィルターは33
×33mm、長さが 150mmの角柱形状でその軸方向に多数の
孔が形成されたハニカム状であり、各孔を形成する隔壁
の厚さは、0.35mm、孔数は 170個／平方インチである。DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment in which the present invention is embodied in the shape of a filter used in an exhaust gas purifying apparatus for an internal combustion engine will be described below in comparison with a comparative example. This filter is 33
It is a rectangular prism with a length of 33 mm and a length of 150 mm, and has a honeycomb shape with many holes formed in the axial direction. The thickness of the partition wall that forms each hole is 0.35 mm, and the number of holes is 170 / square inch. is there.
【００２１】(実施例１)平均粒径が12.4μｍのα−SiＣ
原料粉末70重量部に対し、平均粒径が約 0.5μｍのβ−
SiＣ粉末を30重量部配合し、さらに有機樹脂バインダー
としてメチルセルロース９重量部、分散剤 6.5重量部、
および水21.5重量部を配合して均一に混合し、原料組成
物を調製した。そして、この原料組成物を押し出し成形
機に充填し、押し出し速度40cm／min.にて上記形状のハ
ニカム成形体を成形し、酸素濃度５％、昇温速度15℃／
min.、400 ℃×60min.の条件で脱脂処理した。このとき
の熱分解炭素含有率は1.20重量％であった。脱脂が完了
した成形体を焼成炉内に移すと共に、１気圧のアルゴン
ガス雰囲気下、昇温速度５℃／min. (≦1500℃) 、２℃
／min. (≦2200℃) にて加熱を開始し、所定の温度まで
それぞれ昇温し、1500℃×１分、2200℃×４分焼成を施
して、ハニカム状の多孔質SiＣ焼結体を作製した。これ
らのSiＣ焼結体の一部を切り出し、３点曲げ強度、平均
気孔径、気孔率を試験した。その結果を表１に示す。な
お、前記ハニカム状フィルターの３点曲げ強度は、下部
スパン間隔 135mm、ヘッドスピード５mm／min.の条件
で、下記計算式を用いて算出した。 Ｋ＝（Ｐ×Ｌ）／（４×Ｚ） 上記式において、Ｋは３点曲げ強度、Ｐは荷重、Ｌは下
部スパン間隔、Ｚは断面二次モーメントであり、断面二
次モーメントの値は2500を用いた。Example 1 α-SiC having an average particle size of 12.4 μm
For 70 parts by weight of the raw material powder, β-
30 parts by weight of SiC powder were mixed, 9 parts by weight of methylcellulose as an organic resin binder, 6.5 parts by weight of a dispersant,
And 21.5 parts by weight of water were mixed and uniformly mixed to prepare a raw material composition. Then, this raw material composition was filled into an extrusion molding machine, and a honeycomb molded body having the above shape was molded at an extrusion speed of 40 cm / min., An oxygen concentration of 5%, and a temperature rising rate of 15 ° C. /
Degreasing was performed under the conditions of min., 400 ° C. × 60 min. At this time, the pyrolytic carbon content was 1.20% by weight. The degreased green body is transferred into a firing furnace, and the temperature is increased at a rate of 5 ° C./min. (≦ 1500 ° C.) at 1 atm in an argon gas atmosphere.
/ Min. (≦ 2200 ° C), heating to predetermined temperatures, firing at 1500 ° C x 1 minute and 2200 ° C x 4 minutes to obtain a honeycomb-shaped porous SiC sintered body. Produced. A part of these SiC sintered bodies was cut out, and three-point bending strength, average pore diameter, and porosity were tested. Table 1 shows the results. The three-point bending strength of the honeycomb filter was calculated using the following equation under the conditions of a lower span interval of 135 mm and a head speed of 5 mm / min. K = (P × L) / (4 × Z) In the above equation, K is the three-point bending strength, P is the load, L is the lower span interval, Z is the second moment of area, and the value of the second moment of area is 2500 was used.
【００２２】[0022]
【表１】 [Table 1]
【００２３】(実施例２)前記実施例１におけるのと同じ
原料粉末を使用し、脱脂条件を変えて前記実施例と同様
にしてハニカム状の多孔質SiＣ焼結体を作製した。これ
らの多孔質焼結体の特性を表１に示す。Example 2 A honeycomb-shaped porous SiC sintered body was produced in the same manner as in Example 1 except that the same raw material powder as in Example 1 was used and degreasing conditions were changed. Table 1 shows the characteristics of these porous sintered bodies.
【００２４】(実施例３)前記実施例における原料粉末の
配合に代え、出発原料として平均粒径が約 3.6μｍのα
−SiＣ粉末90重量部に対し、平均粒径が約0.72μｍのβ
−SiＣ粉末を10重量部配合したものを使用し、脱脂条件
を変えて前記実施例と同様にしてハニカム状の多孔質Si
Ｃ焼結体を作製した。これらの多孔質焼結体における特
性を前記実施例と同様に測定を行なった。その結果を表
２に示す。(Example 3) In place of the mixing of the raw material powder in the above-mentioned example, α as an starting material having an average particle size of about 3.6 μm was used.
-Β of an average particle size of about 0.72 μm with respect to 90 parts by weight of SiC powder.
Using a mixture of 10 parts by weight of SiC powder, changing the degreasing conditions, and forming a honeycomb-like porous Si
A C sintered body was produced. The characteristics of these porous sintered bodies were measured in the same manner as in the above examples. Table 2 shows the results.
【００２５】[0025]
【表２】 [Table 2]
【００２６】(実施例４〜６)前記実施例における原料粉
末の配合に代え、出発材料として平均粒径が約4.77μｍ
のα−SiＣ原料粉末90重量部に対し、平均粒径が約0.73
μｍのβ−SiＣ原料粉末を10重量部配合したものを使用
し、脱脂条件を変えて前記実施例と同様にしてハニカム
状の多孔質SiＣ焼結体を作製した。これらの焼結体にお
ける多孔質体の特性を前記実施例と同様に測定を行なっ
た。その結果を表３に示す。(Examples 4 to 6) Instead of the compounding of the raw material powder in the above example, the starting material had an average particle size of about 4.77 μm.
90 parts by weight of α-SiC raw material powder having an average particle size of about 0.73
A honeycomb-shaped porous SiC sintered body was produced in the same manner as in the above-mentioned example, using a mixture of 10 parts by weight of a β-SiC raw material powder of μm and changing the degreasing conditions. The characteristics of the porous bodies in these sintered bodies were measured in the same manner as in the above-mentioned examples. Table 3 shows the results.
【００２７】[0027]
【表３】 [Table 3]
【００２８】(比較例)前記実施例における原料配合で脱
脂条件を変え、前記実施例と同様にしてハニカム状の多
孔質SiＣ焼結体を作製した。これらの焼結体における平
均気孔径を前記実施例と同様に測定を行なった。その結
果を表１〜表３にあわせて示す。(Comparative Example) A honeycomb-shaped porous SiC sintered body was produced in the same manner as in the above example, except that the degreasing conditions were changed by mixing the raw materials in the above example. The average pore diameter of these sintered bodies was measured in the same manner as in the above example. The results are shown in Tables 1 to 3.
【００２９】これらの結果から、脱脂条件または配合す
るα−SiＣ粉末, β−SiＣ粉末の量もしくは粒径を適宜
設定することにより、高強度で多孔質なα−SiＣ焼結体
を容易かつ確実に製造できることがわかる。From these results, it is possible to easily and reliably produce a high-strength, porous α-SiC sintered body by appropriately setting the degreasing conditions or the amounts or particle diameters of the α-SiC powder and β-SiC powder to be mixed. It can be seen that it can be manufactured.
【００３０】[0030]
【発明の効果】以上詳述したように本発明によれば、高
強度多孔質α−SiＣ焼結体を容易かつ確実に製造するこ
とができると共に、気孔の大きさが比較的均一で、機械
的強度に優れた焼結体を安価に製造することができる。As described above in detail, according to the present invention, a high-strength porous α-SiC sintered body can be easily and reliably produced, and the pore size is relatively uniform. A sintered body having excellent mechanical strength can be manufactured at low cost.
Claims (2)
が 0.3〜50μｍのSiＣ原料粉末と有機樹脂バインダーと
を混合して成形し、その成形体を酸素含有率が１〜10％
の雰囲気中において該成形体中の熱分解炭素の含有率が
0.5〜５重量％となるように加熱した後、該成形体を15
00〜2500℃の非酸化性雰囲気中で焼成することを特徴と
する高強度多孔質α−SiＣ焼結体の製造方法。1. An SiC raw material powder having an SiO 2 content of 0.1 to 5% by weight and an average particle diameter of 0.3 to 50 μm is mixed with an organic resin binder and molded, and the molded product is mixed with an oxygen content of 1 to 10%. %
In the atmosphere of the above, the content of pyrolytic carbon in the molded body is
After heating to 0.5 to 5% by weight, the molded body is
A method for producing a high-strength porous α-SiC sintered body, characterized by firing in a non-oxidizing atmosphere at 00 to 2500 ° C.
有率が60〜100 ％の粉末を用いることを特徴とする請求
項１に記載の製造方法。2. The method according to claim 1, wherein a powder having a content of α-SiC of 60 to 100% is used as the SiC raw material powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33216796A JP3983838B2 (en) | 1996-12-12 | 1996-12-12 | Method for producing high-strength porous α-SiC sintered body |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33216796A JP3983838B2 (en) | 1996-12-12 | 1996-12-12 | Method for producing high-strength porous α-SiC sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10167854A true JPH10167854A (en) | 1998-06-23 |
| JP3983838B2 JP3983838B2 (en) | 2007-09-26 |
Family
ID=18251911
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33216796A Expired - Lifetime JP3983838B2 (en) | 1996-12-12 | 1996-12-12 | Method for producing high-strength porous α-SiC sintered body |
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| Country | Link |
|---|---|
| JP (1) | JP3983838B2 (en) |
Cited By (10)
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|---|---|---|---|---|
| JP2001064084A (en) * | 1999-07-21 | 2001-03-13 | Inst Fr Petrole | Honeycomb monolithic structure of fine pore ceramic material and its use as particle filter |
| JP2001524451A (en) * | 1997-12-02 | 2001-12-04 | コーニング インコーポレイテッド | Method for firing ceramic honeycomb body |
| JP2006001799A (en) * | 2004-06-18 | 2006-01-05 | National Institute For Materials Science | Method for manufacturing silicon carbide porous body |
| WO2006007950A1 (en) * | 2004-07-21 | 2006-01-26 | Fachhochschule Koblenz | Batch for producing a fireproof ceramic moulded body, method for the production of the same and use thereof as a diesel particulate filter |
| WO2008032390A1 (en) * | 2006-09-14 | 2008-03-20 | Ibiden Co., Ltd. | Process for producing honeycomb structure |
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|---|---|---|---|---|
| JP4771590B2 (en) * | 1997-12-02 | 2011-09-14 | コーニング インコーポレイテッド | Method for firing ceramic honeycomb body |
| JP2001524451A (en) * | 1997-12-02 | 2001-12-04 | コーニング インコーポレイテッド | Method for firing ceramic honeycomb body |
| JP2001064084A (en) * | 1999-07-21 | 2001-03-13 | Inst Fr Petrole | Honeycomb monolithic structure of fine pore ceramic material and its use as particle filter |
| JP2006001799A (en) * | 2004-06-18 | 2006-01-05 | National Institute For Materials Science | Method for manufacturing silicon carbide porous body |
| WO2006007950A1 (en) * | 2004-07-21 | 2006-01-26 | Fachhochschule Koblenz | Batch for producing a fireproof ceramic moulded body, method for the production of the same and use thereof as a diesel particulate filter |
| JP2009505933A (en) * | 2005-08-23 | 2009-02-12 | ダウ グローバル テクノロジーズ インコーポレイティド | An improved method for removing binders from ceramic honeycombs. |
| EP1902766A1 (en) | 2006-09-14 | 2008-03-26 | Ibiden Co., Ltd. | Method for manufacturing honeycomb structured body |
| JP2009112880A (en) * | 2006-09-14 | 2009-05-28 | Ibiden Co Ltd | Manufacturing method of honeycomb structure |
| WO2008032390A1 (en) * | 2006-09-14 | 2008-03-20 | Ibiden Co., Ltd. | Process for producing honeycomb structure |
| EP2105424A1 (en) * | 2008-03-27 | 2009-09-30 | Ibiden Co., Ltd. | Method for manufacturing honeycomb structured body |
| CN102924084A (en) * | 2012-11-22 | 2013-02-13 | 中原工学院 | Method for preparing silicon carbide ceramic product by adopting pre-oxidizing process |
| WO2016052469A1 (en) * | 2014-09-29 | 2016-04-07 | イビデン株式会社 | Honeycomb filter and method for manufacturing same |
| JP2016067995A (en) * | 2014-09-29 | 2016-05-09 | イビデン株式会社 | Honeycomb filter and manufacturing method for the same |
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